Potassium Carbonate → 1,5-Dichloro-2-fluoro-3-(3,3,3-trifluoroprop-1-en-2-yl)benzene

1-bromo-3,5-dichloro-2-fluorobenzene (10 g), (3,3,3-trifluoroprop-1-en-2-yl)-boronic acid (7.5 g) and potassium carbonate (13.6 g) were dissolved in tetrahydrofuran (41 ml) and water (20 ml), and then deaerated. Dichlorobis(triphenylphosphine)palladium (II) (1.4 g) was added thereto and the mixture was stirred for 3 hours under reflux under argon atomosphere. After cooling the mixture to the room temperature, water and n-hexane were added, and the organic layer was washed with water and dried over anhydrous magnesium sulfate. The drying agent was filtered off, the solvent was distilled off under reduced pressure, and the residue was roughly purified by silica gel chromatography (n-hexane) to obtain a mixture containing 1,3-dichloro-2,4-difluoro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzene and hexane.

1. temperatureunder reflux under argon atomosphere
2. additionwere added
3. washthe organic layer was washed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationThe drying agent was filtered off
6. distillationthe solvent was distilled off under reduced pressure
7. customthe residue was roughly purified by silica gel chromatography (n-hexane)
8. customto obtain a mixture

ORDレコード

ord-371fd72d8e624aa7a9fb9e25e228fb37

出典データセット

uspto-grants-2016_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09375000B2